AKWA IBOM STATE UNIVERSITY

Department of Chemical/Petrochemical Engineering

CHEMICAL ENGINEERING PROCESS DESIGN II

1
PLANT DESIGNFOR THE PRODUCTION OF 30,000 KILOGRAM PER ANUM OF

ZEOLITE FROM KAOLIN

Written By

Okpo, Emmanuel Amba

AK16/ENG/CPE/051

Akpan, Anthonia Athanasius

AK14/ENG/CPE/006

A Plant Design Project Submitted to the Department of

Chemical/Petrochemical Engineering, AkwaIbom State University, MkpatEnin LGA in

Partial Fulfilment of the Requirement for the Award of Bachelor of

Engineering (B.ENG) in Chemical/Petrochemical Engineering

June, 2022

2
 Executive Summary

The manufacture of zeolite from kaolin clay conversion is depicted in this plant design, which has a capacity of
30,000kg annually. The plant's capacity is determined by evaluating the return on investment and net present
worth of numerous possible capacities. Different trends were applied to historical demand data to anticipate
capacity. The Zeolite 5A molecular sieves are used to separate normal and isoparaffins from sour natural gas,
removing water, carbon dioxide, and hydrogen sulfide while reducing COS production. An estimate of the
overall capital investment will be made. The factory is expected to generate $20 million in annual net profit. The
design prioritizes maximizing safety and minimizing environmental effect while being profitable. In general,
synthesis experiments are neither complicated nor dangerous, and standard chemical laboratory precautions are
sufficient to safeguard both the equipment and the researcher. However, the inexperienced user should be
warned about a few hazards. From 2022 to 2030, the global zeolite market is estimated to develop at a
compound annual growth rate (CAGR) of 6.2 percent. Over the forecast period, the market is expected to rise
due to rising investments in growing petrochemical production and expansion in the detergents industry.
Zeolites are commonly employed in the petrochemicals sector as a catalyst for accelerating chemical reactions
due to their stability, excellent activity, and selectivity in conversion processes. Furthermore, because of their
high absorption capacity for liquid components, zeolites are frequently used in the detergent manufacturing
process, resulting in increased zeolites demand.

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 Table of Contents
Executive Summary...................................................................................................................3

Certification................................................................................................................................4

Dedication..................................................................................................................................5

Acknowledgment.......................................................................................................................6

CHAPTER ONE........................................................................................................................8

INTRODUCTION......................................................................................................................8

1.1 Background of Studies...................................................................................................8

1.2 Problem Statement.........................................................................................................9

1.3 Aim...............................................................................................................................10

1.4 Objectives.....................................................................................................................10

1.5 Scope of the Design.....................................................................................................10

CHAPTER TWO.....................................................................................................................11

LITERATURE REVIEW.........................................................................................................11

2.1 Review of Previous Designs........................................................................................11

2.1.1 Clay conversion process (Kaolin conversion process).........................................12

2.2 Extent of Past Designs.................................................................................................13

2.3 Limitations of Previous Designs...................................................................................15

2.4. Modified Design...........................................................................................................15

CHAPTER THREE..................................................................................................................16

3.1. Process Description...........................................................................................................16

3.2.1 Material Balance Over Mixer 1...................................................................................17

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 3.2.3 Material Balance Over Zeolite Formation Reactor.....................................................18

3.2.4 Material Balance Over Mixer 3...................................................................................19

3.2.5 Material Balance Over Zeolite 5A Formation Reactor...............................................19

3.2.5 Material Balance Over Zeolite 5A-Dry Formation Reactor.......................................19

3.2.6 Material Balance Over Dryer......................................................................................21

3.2.7 Material Balance Over Screen....................................................................................21

3.3. Energy Balance.................................................................................................................22

3.2.1 Energy Balance Over Mixer1......................................................................................22

3.2.2 Energy Balance Over Mixer2......................................................................................22

3.2.3 Energy Balance Over Mixer3......................................................................................23

3.2.3 Energy Balance Over Zeolite 4A Formation Reactor.................................................23

3.2.4 Energy Balance Over Zeolite 5A Formation Reactor.................................................23

3.2.5 Energy Balance Over Zeolite 5A-Dry Formation Reactor.........................................24

3.2.6 Energy balance Over Dryer.........................................................................................24

3.2.7 Energy balance Over Screen.......................................................................................25

3.2.8 Energy balance Over Kiln...........................................................................................25

3.2.9 Energy balance Over Screen2.....................................................................................25

CHAPTER 4.............................................................................................................................26

EQUIPMENT DESIGN...........................................................................................................26

4.1. Rstoic Reactor (Conversion Reactor)................................................................................26

4.2. Dryer.................................................................................................................................27

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 4.2.1 The description of dryer classification criteria is:.......................................................27

4.2.2 Calculation of Heat Duty............................................................................................27

4.2.3 Calculation of Inside Diameter and Length................................................................29

4.2.4 Calculation of RPM, Flight Design and Residence Time...........................................32

4.2.5 Calculation of Shell Dryer Thickness and Outer Diameter........................................33

4.2.6 Calculation of the Insulation Thickness......................................................................34

4.2.7 Calculation of the Live Load and Rotating Load........................................................35

4.2.8 Calculation of Blower Power, Motive Power and Power to Drive a Dryer................36

CHAPTER 5.............................................................................................................................39

SIMULATION.........................................................................................................................39

5.1 Simulation Software...........................................................................................................39

5.2. Selection of Fluid Package................................................................................................39

5.3. Process Conditions............................................................................................................39

5.4. Process Simulation............................................................................................................44

CHAPTER 6.............................................................................................................................54

PROCESS CONTROL AND INSTRUMENTATION............................................................54

6.1 OBJECTIVES....................................................................................................................54

6.2 Selection of Controllers.................................................................................................54

6.3 Core Technical Aspects to be Determined Before Selecting a Control System...........58

6.3.1 Temperature Indicating Controller........................................................................59

CHAPTER 7.............................................................................................................................60

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EQUIPMENT COST AND ECONOMIC EVALUATION....................................................60

7.1 Equipment Cost.............................................................................................................60

7.1.1 Cost of Reactor......................................................................................................61

7.1.2 Cost of Dryer.........................................................................................................62

7.1.3 Cost of Screen........................................................................................................64

7.1.4 Summary of Costing for the Plant...............................................................................65

7.1.4 Utility Cost..................................................................................................................65

7.1.5 Installation Cost..........................................................................................................66

7.2. Economic Evaluation....................................................................................................67

7.2.1 Production Cost......................................................................................................67

7.2.2 Estimation of Fixed Capital Cost...........................................................................68

7.2.3 Estimation OF Working Capital............................................................................69

7.2.4 Total Investment and Return in Investment...........................................................69

CHAPTER EIGHT...................................................................................................................71

8.1 Safety.............................................................................................................................71

8.2 HAZOP........................................................................................................................74

8.3 Environmental Impact Assessment (EIA).....................................................................77

CHAPTER 9.............................................................................................................................79

CONCLUSION AND RECOMMENDATION.......................................................................79

REFERENCES.........................................................................................................................80

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 Certification

I hereby certify the contents of this Plant design project by Okpo, Emmanuel Amba
[AK16/ENG/CPE/051] and Akpan, Anthonia Athanasius [AK16/ENG/CPE/006], of the
department of Chemical/Petrochemical Engineering.

Name: Okpo, Emmanuel Amba Name: Akpan, Anthonia Athanasius

Signature: __________________ Signature: __________________

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 Dedication

I dedicate this report to God almighty for his unlimited grace, consistent love, and
immeasurable faithfulness and for sparing my life throughout our stay in the university, and
to our sponsors and good friends who gave us all the support I needed.

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 Acknowledgment

We would like to express our special thanks of gratitude to our lecturer Engr. Umo Aniediong

as well as our H.O.D Dr Rasheed Babalola, who gave us the opportunity to carry out the plant

design. This plant design also helped us in doing a lot of research and we came to know about

so many new things about simulation.

We are extremely grateful to our parents, and our friends, most especially our colleague

Treasure Nse Bassey, Elijah Edok James and John Akpan who gave valuable suggestion and

support. This cooperation and healthy criticism can handy and useful with them. Hence, I

would like to thank all the above mentioned people once again.

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 List of Figures

Figure 2.1 The mineral stilbite (left) and the crystal structure (framework) of the stilbite

group (right)

Figure 2.2 Early discoveries of zeolite materials and their characteristics, the beginning of the

modern zeolite science, and their industrial applications

Figure 2.3 The Process Flow diagram of zeolite

Figure 5.1 Screenshot of Mass/Heat transfer of dryer

Figure 5.2 Screenshot of Specification of dryer

Figure 5.3 Screenshot of the setting of mixer1

Figure 5.4 Screenshot of the setting of kiln

Figure 5.5 Screenshot of the setting of mixer 3

Figure 5.6 Screenshot of the setting of Mixer 2

Figure 5.7 Screenshot of the specification of screen1

Figure 5.8 Screenshot of the specification of screen2

Figure 5.9 Screenshot of PSD of zeolite 4A formation reactor

Figure 5.10 Screenshot of Heat of Reaction of Zeolite 4A formation reactor

Figure 5.11 Screenshot of reaction tab of zeolite4A formation reactor

Figure 5.12 Screenshot of specification of zeolite4A formation reactor

Figure 5.13 Screenshot of PSD of zeolite 5A formation reactor

Figure 5.14 Screenshot of reaction tab of zeolite 5A formation reactor

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Figure 5.15 Screenshot of the specification of zeolite 5A dry formation reactor

Figure 5.16 Screenshot of the PSD of zeolite 5A dry formation reactor

Figure 5.17 Screenshot of the specification of zeolite 5A dry formation reactor

Figure 5.18 PFD of actual zeolite 5A production.

Figure 7.1 Based on purchase cost of miscellaneous equipment, cost factors for use. Cost

basis mid 2004

Figure 7.2 Dryer cost estimates

Figure 7.3 Cost estimates for screen

Figure 7.4 Summary of production cost

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 List of Tables

List of T

Table 3.1: Material Balance over Mixer 1

Table 3.2: Material Balance over Mixer 2

Table 3.3: Material Balance over Zeolite 4A Formation Reactor

Table 3.4: Material Balance over Mixer 3

Table 3.5: Material Balance over Zeolite 5A Formation Reactor

Table 3.6: Material Balance over Zeolite 5A-Dry Formation Reactor

Table 3.7: Material Balance over Dryer

Table 3.8: Material Balance over Screen

Table 3.9: Energy Balance over Mixer1

Table 3.10: Energy Balance over Mixer2

Table 3.11: Energy Balance over Mixer3

Table 3.12: Energy Balance Over Zeolite 4A Formation Reactor

Table 3.13: Energy Balance Over Zeolite 5A Formation Reactor

Table 3.14: Energy balance over Zeolite 5A-Dry Formation Reactor

Table 3.15: Energy balance Over Dryer

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Table 3.16: Energy balance Over Screen

Table 3.17: Energy balance Over Kiln

Table 3.18: Energy balance Over Screen 2

Table 4.1: Process conditions of the dryer

Table 5.1: Process Condition of Mixer1

Table 5.2: Process Condition of Mixer2

Table 5.3: Process Conditions for Zeolite 4A Formation Reactor

Table 5.4: Process Conditions for Mixer3

Table 5.5: Process Conditions for Zeolite 5A Formation Reactor

Table 5.6: Process Conditions for Zeolite 5A-Dry Formation Reactor

Table 5.7: Process Conditions for Dryer

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 CHAPTER ONE

INTRODUCTION

1.1 Background of Studies

Zeolites are crystalline aluminosilicates earth minerals comprising of a three dimensional

network of SiO4 and AIO4- tetrahedral of open structures with cations positioned within

materials pore with diameters of molecular dimensions (0.3 to 1.4 nm) (Olaremu et al., 2018;

Abdullahi et al., 2017). They are formed under hydrothermal conditions and were first

recognized as a new type of mineral in 1756 (Farag and Zhang, 2018). Currently, there are

some 40 different natural zeolites and roughly 150 synthetic zeolites (Abdullahiet al., 2017).

Most commercial zeolites are high purity synthetic products made from inorganic materials.

There are several types of building units present in zeolite frameworks. The primary building

unit (PBU) is the tetrahedral unit, while the secondary building units (SBU) are the molecular

complexes which are formed by the PBU element. The SBUs consist of single and double

rings of tetrahedral, which can be further assembled into different types of structural units,

the so-called Common Building Unit (CBU). These CBUs are double 6-ring, alpha-cavities,

which are useful in characterizing similarities between framework types (Shuai, 2009).

Zeolites can selectively absorb or reject molecules based on differences in shape and other

properties. These characteristics have resulted in a variety of uses for zeolites. such as water

softening in detergents (replacing undesirable polyphosphates), absorbents for oil in

industrial spills, gas separation, water filtration, and heavy metal removal in water

purification and wastewater treatment. The major application of zeolite is in the petroleum

industry, where it is used as a catalyst for fluid catalytic cracking. Industrial estimates of

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worldwide sales of zeolite FCC catalysts are approximately $1 billion per year and constitute

a major portion of the $2.16 billion worldwide refinery catalyst market (Olaremuet al., 2018).

Zeolite catalysts have been the source of major improvements in gasoline yield and octane as

well as in the production of cleaner fuels and lubricants with enhanced performance

(Olaremuet al., 2018). The zeolite Y continues to provide the greatest gasoline yield at the

highest octane with the greatest degree of catalytic stability. Various applications of zeolite

have led to the need to increase production at a low cost (Ahmed et al., 2018).

Kaolin clay offers a unique, environmentally friendly, and sustainable route toward the

manufacturing of zeolite. Kaolin-based zeolites are produced from natural and cheap

resources as against the conventional process that employs pure sodium silicate and sodium

aluminate, which are expensive with a negative impact on the environment and hence not

sustainable (Abdullahiet al., 2017). Kaolinite is a clay mineral with a 1:1 clay layer and the

structural formula Al4Si4O10(OH)8, with a theoretical chemical composition of 46.54%

SiO2, 39.50% Al2O3, and 13.96% H2O (Murray, 2007).

Basically, there are two steps in producing zeolite from kaolin: metakaolinization, which

involves transforming kaolin to metakoalin by chemically activating kaolin clay; and

zeolinization, which involves the hydrothermal treatment of the metakaolin with an aqueous

alkali solution to form the required zeolite.

1.2 Problem Statement

The conventional process employs pure sodium silicate and sodium aluminate for the

synthesis of zeolite, which are expensive with a negative impact on the environment and

hence not sustainable as their application ranges from petroleum refining to waste treatment,

so the need to increase the production rate increases.

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1.3 Aim

This research work is aimed at designing a plant for the production of 30,000 kilogram per

annum of zeolite from kaolin clay.

1.4 Objectives

1. To develop simulation for the production of zeolite from kaolin using ASPEN PLUS.

2. To write material and energy balance for process.

3. To carry out equipment design for each unit operations in the process.

4. To carry out control and instrumentation.

5. To perform economic costing and evaluation of the process.

6. To conduct HAZOP analysis for plant and environmental safety.

1.5 Scope of the Design

The focus of this research is to approach the objectives of more efficient and economically

more viable zeolite production.

Kaolin clay offers a unique, environmentally friendly, and sustainable route toward the

manufacturing of zeolite. Kaolin-based zeolites are produced from natural and cheap

resources as against the conventional process that employs pure sodium silicate and sodium

aluminate, which are expensive with a negative impact on the environment and hence not

sustainable.

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 CHAPTER TWO

LITERATURE REVIEW

2.1 Review of Previous Designs

Synthesis of zeolite through the hydrothermal route is a multiphase reaction-crystallization

process, usually encompassing at least one liquid phase and both amorphous and crystalline

solid phases (Abdullahiet al., 2017). (Flanigen, 2001): An alternative zeolite synthesis route

based on fluoride-containing compositions as mineralizing media has been reported by

(Flanigen, 2001). Nevertheless, (Cundy and Cox, 2003) maintained that the major synthesis

route for many zeolites and zeotypes is the hydrothermal process.

Kaolin clay offers a unique, environmentally friendly, and sustainable route toward the

manufacturing of zeolite. Kaolin-based zeolites are produced from natural and cheap

resources as against the conventional process that employs pure sodium silicate and sodium

aluminate, which are expensive with a negative impact on the environment and hence not

sustainable (Abdullahiet al., 2017).

Previous work has shown that the improvement of the properties of kaolinite by chemical

methods is difficult due to its low reactivity. This clay mineral is not significantly affected by

acid or alkaline treatments, even under strong conditions (Reyes et al., 2010). Therefore, it is

usually used after calcination at temperatures between 550 and 950 °C to obtain a more

reactive phase (metakaolinite) under chemical treatments, with the loss of structural water

and reorganization of the structure (Farag, 2012). Only a small portion of the AlO6

octahedral structure is preserved, with the remainder being converted into much more

reactive tetra- and penta-coordinated units (Reyes et al., 2010). Several authors have

18
discussed the optimal conditions for producing a highly reactive metakaolinite, reporting

temperatures ranging from 600 to 800 °C. Calcination at higher temperatures leads to the

formation of mullite and cristobalite (Abdullahiet al., 2017). Several authors have reported

the synthesis of metakaolinite-based zeolitic materials.

2.1.1 Clay conversion process (Kaolin conversion process)

Basically, there are two steps in producing zeolite from kaolin: metakaolinization and

Zeolinization.

A. Metakaolinization

Metakaolinization involves transforming kaolin(Al2Si2O5(OH)4) to metakoalin(Al2Si2O7) by

chemically activating kaolin clay.This is done by air calcinations at 500 – 600 °C, to form

meta-kaolin according to the reaction.

Al2Si2O5(OH)4 → Al2Si2O7 + 2H2O (at 550 °C)

At high temperature (1000 – 1100 °C) the meta-kaolin is broken down to calcined kaolin,

called mullite (Si2Al6O13), and SiO2 called cristobalite.

3Al2Si2O7 → Si2Al6O13 + 4SiO2 (at 1000-1100°C)

B. Zeolinization

Zeolinization involves the hydrothermal treatment of the metakaolin with aqueous alkali

solution to form the required zeolite.

Farag in 2012 simulated a process of zeolite 4A and 5A manufacture from kaolin by the basic

process of metakaolinization and zeolinization. He reacted mullite and cristobalite with

caustic soda and water in a gel make-up tank to produce zeolite 4A gel.

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12NaOH + 204H2O + Si2Al6O13 + 4SiO2 (200 F) → 3(2Na2O+Al2O3+2SiO3+70 H2O) Zeolite

4A Gels

To produce zeolite 5A, zeolite 4A gel is fed to an ion exchanger, where it is mixed with

calcium chloride and water. In this process some of Na + ions in zeolite 4A gel are replaced by

calcium ions, Ca2+.

(2Na2O+Al2O3+2SiO2+70H2O) (Zeolite 4A Gel) + 0.7 CaCl 2 (200 F) →

0.7CaO+0.3Na2O+Al2O3+2SiO2+70H2O (Zeolite 5A wet) + Na2O + 1.4NaCl

Wet zeolite 5A will pass through dryer to remove part of the water and form the dry zeolite at

1000℉.

0.7CaO+0.3Na2O +Al2O3+2SiO2+70H2O (1000℉) → 65.5H2O + 0.7CaO+0.3Na2O

+Al2O3+2SiO2+4.5H2O (Zeolite 5A dry)

The zeolite 5A dryer product has a particle size distribution which has to be incorporated into

the process simulation model.

2.2 Extent of Past Designs

Zeolite materials were discovered in the eighteenth century when a Swedish chemist, founder

of modern mineralogy, Baron Axel Fredrik Cronstedt, discovered that during the heating of

mineral “stilbite,” moisture appears on its surface. His discovery began the research of

chemical, physical, and mineralogical characteristics of natural zeolites.

In spite of the limited capabilities of structural research of zeolites at the time of their

discovery (unlike today’s modern methods), researchers set the foundations for today’s

application of natural and synthetic zeolites (Figure 1). Based on Cronstedt’s observations

and research, in the middle of the nineteenth century according to the available literature, the

first synthetic zeolite-levinite (Annales des mines, 1999) was synthesized, while in the first

20
half of the twentieth century (after the first structural analysis of zeolite materials), a

synthetic analog zeolite-mordenite (Pramod K et al, 1978) was synthesized. Intensive

research on the synthesis as well as physical and chemical properties of zeolites (absorption,

ion exchange, dehydration) enabled the industrial application of zeolites. Significant

discoveries and research of zeolites, as well as the beginning of modern zeolite science

(parallel with the development of new instrumental techniques), are shown in Figure 2.

Figure 2.1 The mineral stilbite (left) and the crystal structure (framework) of the stilbite

group (right)

Figure 2.2 Early discoveries of zeolite materials and their characteristics, the beginning of the

modern zeolite science, and their industrial applications

21
Currently, the publication materials for simulation design of the production of zeolites from

kaolin clay is limited to laboratory and experimental work. But Farag (2012) developed the

design and simulation of synthetic zeolite-4A and 5A manufacturing for green processing

through hydrogel process and kaolin clay.

Figure 2.3 The Process Flow diagram of zeolite

2.3 Limitations of Previous Designs

The previous design of producing zeolites from kaolin clay had the limitation of modelling

kaolin, zeolite 4A, and zeolite 5A as non-conventional without providing their component

attributes with necessary data for modelling non-conventional components. The flowsheet did

not include the dihydroxylation of kaolin; mullite and cristobalite were reacted with caustic

soda and water in a gel make-up tank to produce 4A gel instead.

2.4. Modified Design

The computer simulation and design for the production of zeolite from kaolin clay was

modified by providing appropriate atomic mass balance to flag off error in the chemical

balance.

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 CHAPTER THREE

MATERIAL AND ENERGY BALANCE

3.1. Process Description

This process begins with kaolin (Al2Si2O5(OH)4), which is usually dehydroxylated to

metakaolinn. This is accomplished by air calcination at 500–600°C to produce meta-kaolin in

accordance with the reaction;

Al2Si2O5(OH)0 Al2SiO7 + 2H2O (at 550oC)

Kaolin Meta-kaolin

At high temperatures (1000 to 1100oC) the meta-kaolin is broken down into calcinated

kaolin, called mullite (Si2Al6O13) and SiO2, called cristobalite.

3Al2Si2O7 Si2Al6O13 + 4SiO2 (at 1000 – 1100oC)

The process flow diagram below shows the meta-kaolinization pellet (mullite and

cristobalite) reacting with caustic soda and water in a reactor to produce zeolite 4A gel with

the conversion reaction:

12NaOH + 204H2O + Si2Al6O13 + 4SiO2 (200oF) 3(2Na2O-Al2O3-2SiO3-70H2O)

Zeolite 4A gels

Zeolite 4A gel was fed to another model ion exchanger reactor, where it was mixed with

calcium chloride and water to create zeolite 5A. Some of the Na+ ions in the zeolite 4A gel

was replaced by calcium ions, Ca2+, throughout this process. The reaction was as follows:

23
(2Na2O-Al2O3-2SiO3-70H2O) (Zeolite 4A gel) + 0.7CaCl2 (200oF) 0.7CaO-

0.3Na2O-Al2O3-2SiO2-70H2O (Zeolite 5A wet) + Na2O + 1.4NaCl

In the third reactor, wet zeolite 5A will be transformed to dry zeolite 5A by removing some

of the water before drying it further to produce a high yield of zeolite 5A. The reaction was

0.7CaO-0.3Na2O-Al2O3-2SiO2-70H2O 65.5H2O + 0.70CaO-0.3Na2O-Al2O3-2SiO2-

4.5H2O (Zeolite 5A dry)

The particle size distribution (PSD) of the zeolite 5A dryer product was included in the

process simulation model. To eliminate undersized and large particles, the dryer product is

placed into the screens. The first batch of zeolite 5A (with PSD) leaves the screens.

3.2. Material Balance: Material balance is simply accounting for material. Thus, material

balance of each unit operation are stated below to account for the flow rates of different

streams entering and leaving the chemical or physical processes in the plant.

3.2.1 Material Balance Over Mixer 1

NaOH
MIXER Mix2-Fed
H2O

Table 3.1: Material Balance over Mixer 1

Total Units In Out

Mole kmol/hr 154 154

Mass kg/hr 5060.46344 5060.46344

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3.2.2 Material Balance Over Mixer 2 Mix2 Fed

Pellets
MIXER
H2O RFeed

Table 3.2: Material Balance Over Mixer 2

Total Units In Out

Mole kmol/hr 1957.55387 1957.55387

Mass kg/hr 44903.9313 44903.9313

3.2.3 Material Balance Over Zeolite Formation Reactor

RFeed Zeo-4A
REACTOR

Table 3.3: Material Balance Over Zeolite 4A Formation Reactor

Total Units In Out Generated

Mole kmol/hr 1957.55387 84.1168982 -1873.43697

Mass kg/hr 44903.9313 44903.9313

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3.2.4 Material Balance Over Mixer 3 Cacl2
H2O

ZEO-4A MIX

MIXER

Table 3.4: Material Balance Over Mixer 3

Total Units In Out

Mole kmol/hr 213.154481 213.154481

Mass kg/hr 48903.9313 48903.9313

3.2.5 Material Balance Over Zeolite 5A Formation Reactor

Mix REACTOR Zeo-5A

Table 3.5: Material Balance Over Zeolite 5A Formation Reactor

Total Units In Out Generated

Mole kmol/hr 213.154481 252.599783 39.4453014

Mass kg/hr 48903.9313 48903.9313

3.2.5 Material Balance Over Zeolite 5A-Dry Formation Reactor

REACTOR
Zeo-5A Zeo-5A IN
Table 3.6: Material Balance Over Zeolite 5A-Dry Formation Reactor

26
Total Units In Out Generated

Mole kmol/hr 252.599783 1772.40404 1519.80426

Mass kg/hr 48903.9313 48903.9313

3.2.6 Material Balance Over Dryer AIR-OUT

ROTARY
ZEO-5A IN ZEO5A-DRY
DRYER

AIR-IN

Table 3.7: Material Balance Over Dryer

Total Units In Out Relative difference

Mole kmol/hr 1777.58523 1777.58523 1.28E-16

Mass kg/hr 49053.9313 49053.9313 4.17E-11

3.2.7 Material Balance Over Screen

SCREEN
Feed Overflow

Underflow

Table 3.8: Material Balance Over Screen

27
Total Units In Out Relative difference

Mole kmol/hr 1423.03366 1423.03366 -1.60E-16

Mass kg/hr 30554.241 30554.241 1.36E-12

3.3. Energy Balance: The general energy balance equation is given

Energy balance=Energy input −EnergyOutput

Using the equation above, unit operations energy balances was calculated.

3.2.1 Energy Balance Over Mixer1

Qin MIXER Qout

Table 3.9: Energy Balance Over Mixer1

Total Units QIn QOut

Heat Flow kJ/hr -46494398.14 -46494398.14

3.2.2 Energy Balance Over Mixer2

Qin MIXER Qout

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Table 3.10: Energy Balance Over Mixer2

Total Units QIn QOut

Heat Flow kJ/hr -254840423 -254840423

3.2.3 Energy Balance Over Mixer3

Qin MIXER Qout

Table 3.11: Energy Balance over Mixer3

Total Units QIn QOut

Heat Flow kJ/hr -71609189 -71609189

3.2.3 Energy Balance Over Zeolite 4A Formation Reactor

Qtotal=Qin−Qout

Qtotal=−254840423−(−52600625 ) =−202239798KJ/hr

Table 3.12: Energy Balance Over Zeolite 4A Formation Reactor

Total Units QIn QOut Relative difference

Heat Flow kJ/hr -254840423 -52600625 -0.79359387

3.2.4 Energy Balance Over Zeolite 5A Formation Reactor

Qtotal=Qin−Qout

Qtotal=−71609189−(−81726299 )=10117110KJ/hr

29
Table 3.13: Energy Balance Over Zeolite 5A Formation Reactor

Total Units QIn QOut Relative difference

Heat Flow kJ/hr -71609189 -81726299 0.12379259

3.2.5 Energy Balance Over Zeolite 5A-Dry Formation Reactor

Qtotal=Qin−Qout

Qtotal=−81726299−(−145711166 )=63984867 KJ/hr

Table 3.14: Energy balance over Zeolite 5A-Dry Formation Reactor

Total Units QIn QOut Relative difference

Heat Flow kJ/hr -81726299 -145711166 0.43912123

3.2.6 Energy balance Over Dryer

Qtotal=Qin−Qout

Qtotal=−145707409−(−125907409 ) =−19800000KJ/hr

Table 3.15: Energy balance Over Dryer

Total Units QIn QOut Relative difference

Heat Flow kJ/hr -145707409 -125907409 -0.13588877

30
3.2.7 Energy balance Over Screen

Table 3.16: Energy balance Over Screen

Total Units QIn QOut

Heat Flow kJ/hr -126755936.5 -126755936.5

3.2.8 Energy balance Over Kiln

Table 3.17: Energy balance Over Kiln

Total Units In Out Relative difference

Heat Flow kJ/hr -72473451 -72437451 -0.00049673

3.2.9 Energy balance Over Screen2

Table 3.18: Energy balance Over Screen 2

Total Units In Out Relative difference

Heat Flow kJ/hr -28975123 -28975123 2.71E-13

31
 CHAPTER 4

EQUIPMENT DESIGN

4.1. Rstoic Reactor (Conversion Reactor)

Type of equilibrium reactor consider was a vertical type of reactor.

Using the expression for the volume of a reactor by using the design equation below, we

have;

F Ao
V=
−r A

Where FAO = The molar flow rate

-rA = the rate of reaction or the reaction extent

From our simulation, we have;

FAO = 44,909.9kgmole/hr

-rA = 8.59375

44,903.9 3
V= =5225 m
8.59375

Comparing this value with volume gotten from sizing using ASPEN PLUS;

volume = 4087m3

By substituting the value of volume at the rating tab, our calculated parameters were:

Diameter = 1.0668m

Height of the reactor = 4.572m.

32
4.2. Dryer

Table 4.1: Process conditions of the dryer

Feed
Name Mass Flow Rate Inlet Temperature Outlet Temperature
(S/N) Component [kg/hr] [C] [C]
1 CAO 0 50 99.62
2 NA2O 1438.104688
3 AL2O3 0
4 SIO2 0
5 WATER 29387.43442
6 NACL 1898.466578
7 CACL2 197.3873141
8 NAOH 34.99862969
9 MULLITE 0
10 CRISTOBA 3426.683459
11 ZEO-4A 4143.451405
12 ZEO-5A 0
ZEO5ADR
13 Y 8377.404764
AIR 150 190 99.62

4.2.1 The description of dryer classification criteria is:

1. Form of feed: Wet Zeolite 5A

2. Mode of operation: Continuous operation

3. Heating system: Steam heated air

4. Gas flow pattern in dryer: Concurrent gas flow

4.2.2 Calculation of Heat Duty

Using ambient temperature of 30oC and RH = 93% (Wheather Past 2 Weeks in manila,

Philippines 2015)

33
From Psychometric chart of Perry’s Handbook: Humidity = 0.0252kg of water per kg of dry

air.

Taking the humid heat of Air:

Cs=1.005+ 1.88 H =1.005+1.88 ( 0.0252 )

Cs=1.0524KJ/Kg-K

Calculating for the amount of air needed:

Q 1.98× 107 KJ /hr Kg

m= = =208167.06
Cs ∆ T KJ hr
1.0524 ( 463.15−372.77 ) K
Kg−K

To find humidity of outlet Air:

m vapor
H= + H 30 C
o
m air

133.8868 kg water kg water kg water

H= + 0.0252 =0.0258
208,167.05 kg dry air kg dry air kg air

To find the relative humidity of outlet Air:

Air pressure at 99.62oC = 101324.62Pa

1 kmol
0.0491 kg water ×
18.02 kg
PH2O= =7,387.04 Pa
(
0.0491 kg water ×
1 kmol
18.02 kg )(
+ 1 kg dry Air ×
1 kmol
28.84 kg )
× 101,325 Pa

PH 2O 7,387.04 Pa
RH = ×100 %= × 100 %=7.29 %
Pair 101324.62 Pa

34
Thus the outlet air does not exceed the capacity of the air carry vapour since RH<100%

Allotting an allowance of 20%, for the possible heat losses and due to start-up, shutdown and

cleaning (van’t Land, 2012)

kg
ma= (1.20 )( 208,167.05 )
hr

kg
ma=249,800.46
hr

4.2.3 Calculation of Inside Diameter and Length

The allowable mass velocity of the air ranges from 2000kg/hr-m 2 up to 25,000kg/hr-m2

(McCabe, Harriot, & Smith, 1993). Assuming that the mass velocity of air = 5,000kg/hr-m2

Then, the area of dryer,

kg
249,800.46
hr
A= =49.96 m2
kg
5,000
hr−m2

D i=
√
4 (49.96 m2 )
π
=7.98 m

Drying diameter ranges from 1 to 3m (McCabe, Harriot, & Smith, 1993), thus we used the

computer simulation value of tray area of dryer =3.71614 m2

Such that;

Di=
√ 4 (3.71614 m 2)
π
=2.1752 m

35
Thus, the diameter computer by the simulator was accepted.

The following empirical equation is used to calculate for the overall heat transfer coefficient

from Perry’s Handbook with the index n=0.67 (McCormick, 1962). The k value falls in the

range 3.75 ≤ k ≤5.25 as suggested by AICHE for SI unit (van’t Land, 2012). Assuming

k =4.75 :

n
kG
U a=
D

( )
0.67
kg
4.75 5,000
hr−m2 kJ
U a= =656.91
2.1752 m hr −m 3−k

For the calculation of wet bulb temperature, the most economical operation of rotary dryer

can be achieved for Nt is in general between 1.5 and 2.5 (Mujumdar. 2014). Assuming the

value of N t =2

N t =¿
( T Ain −T w
T Aout −T w )
2=¿
( 463.15−T w
372.77−T w )
¿ 463.15−¿ T w
2=
¿ 372.77−¿ T w

2 ( 5.9209−¿ T w )=6.1381−¿ T w

¿Tw
5.9209−¿T w =3.0691−
2

36
 −1
5.9209−3.0691= ∈T w +¿ T w
2

1
2.8518= ∈T w
2

¿ T w =5.7036

5.7036
T w =e =299.95

T w =299.95 K

Calculating the logarithmic mean temperature difference:

( T Ain −T w )−( T Aout −T w ) ( 463.15−299.95 ) −(372.77−299.95)

(∆T )lm = = =11.99 K
(T Ain −T w ) (463.15−299.95)
¿ ¿
(T Aout −T w ) (372.77−299.95)

(∆T )lm =11.99 K

To calculate the length of the dryer:

Q=U a AL(∆ T )lm

Q 1.98 ×107
L= = =676.47 m
U a A ( ∆T )lm kJ 2
656.91 3
(3.71614 m )(11.99 K )
hr −m −k

Checking L/D ratio:

L 676.47 m
= =¿310.99
D i 2.1752 m

37
L/D ratio is most efficient between 4 and 10 for industrial dryer (Mujumdar, 2014), but the

above diameter and length is beyond the accepted ranges of L/D ratio. Therefore, we assumed

the heat duty should be within the range of 200,000kJ/hr.

200000
L= =6.8330 m
kJ
656.91 3
(3.71614 m2 )(11.99 K )
hr −m −k

L 6.8330 m
= =2.9115 m
D i 2.1752 m

Since the L/D ratio for the assumed duty is within 4 and 10 for industrial dryers, therefore the

above diameter and length can be accepted.

4.2.4 Calculation of RPM, Flight Design and Residence Time

Speed values ranges 0.1 to 0.5m/s (van’t Land, 2012). Assuming the peripheral speed of

rotation to be 0.1m/s.

To calculate the speed of rotation of the dryer:

Periphera l speed
RPM =
Diameter

m 60 s
0.1 ×
s 1min
RPM = =2.76 rpm
2.1752 m

The revolution of a dryer varies between 2-5rpm. Therefore, the above value can be accepted.

Flight design:

No . of flights=3 D , ( D∈feet )

38
 (
No . of flights=3 2.1752 m×
1 ft
0.3048 m )
=21.4094 ≈ 21

Flight Depth:

D 2.1752m
F d= = =0.2719
8 8

F d=0.27 m

Using the following empirical equation for the residence time (in minutes) in dryer as

recommended by AICHE (van’t Land, 2012):

−0.5 −0.5
B=5 d p =5 ( 210 ) =0.3450

0.23 L 2 BLG 0.23 (6.8330 ) 2 ( 0.3450 )( 6.8330 ) ( 5,000 )

τ= + = + =75.99 min
F
( )
0.9 0.9
SN D ( 5 ) ( 4.5892 ) ( 2.1752 ) 416.67
1.3425

τ =75.99 min

Residence time of rotary dryer typically ranges of 5-90 minutes (Couper, Penney, Fair, &

Walas, 2005), therefore the computed value is acceptable.

4.2.5 Calculation of Shell Dryer Thickness and Outer Diameter

Considering the material to be used is carbon steel (SA 285, Grade C) because it can

withstand up to 343.33oC. For operating pressure of 0 psig (14.7 psia), the design pressure is

10 psig (24.7 psia) or 170,253.5714 Pa (Hesse &Rushton, 1975)

Using the following formula for working stress:

Sw =S u × F m × F a × Fr × F s

39
Where: Su: minimum specific tensile strength, 380 MPa (ASME SA285 Grade C, n.d.)

Fm: material factor, 0.92 for Grade C material

Fa: radiographically factor, 1.00 since radiographing is not employed

Fr: stress relieving factor, 1.00 since relieving is not employed

Fs: factor of safety, 0.25 for temperature less than 315.56oC

Sw =380 MPa × 0.92× 1.00× 1.00× 0.25

Sw =84.7 MPa

Using the following equation to calculate shell thickness with a corrosion allowance of

6.35mm (Hesse & Rushton, 1975) and efficiency of the joint 0.70 for double-welded butt

joint since radiographing is not employed (Sinnot, 2005):

PD
t s= +C
2 S w e−P

N 1000 mm
170,253.5714×1.3074 m×
m 2
1m
t s= +6.35
( N
)
2× 87,400,000 2 ×0.70 −170,253.5714 2
m
N
m

t s=8.17 mm

The minimum shell thickness of equipment vessel with 1.0668 – 1.524m diameter is

8.128mm (Couper, Penney, Fair & Walas, 2005), therefore above value can be accepted.

To calculate the outer diameter of the dryer:

40
D o =D i+ 2t s=1.3074+2 8.1717 mm × ( 1m
1000 mm )
D o =1.32m

4.2.6 Calculation of the Insulation Thickness

To limit heat loss an insulation is to be given to the dryer. The chosen insulating material is

brick. From literature, its thermal conductivity equals to 0.72W/m.K. Mild steel however has

a thermal conductivity of 51.9220W/m.K.

2 πL ( T 2−T 1 )
Q=
¿ () ()
r2
r1
+
¿
r3
r2
KA KB

Converting 200,000KJ/hr to Watt, we have 55,555.56Watts

2 π ( 6.8330 m ) ( 463.15 K−372.77 K )

55,555.56 W =
( ) ( )
0.6619 0.6619+ t i
¿ ¿
0.6537 0.6619
+
W W
51.9220 0.72
m.K m. K

¿ ( 0.6619+t i
0.6619 )
=0.72 (
3880.78
55,555.56 )
−2.4 ×10 =0.72 ( 0.0699−2.4 ×10 )
−4 −4

¿ ( 0.6619+t i )=0.0502× 0.6619=0.0332

0.6619+t i=e 0.0322 =1.0327

t i=1.0327−0.6619=0.3708

t i=0.3708 m=370.82 mm

41
To calculate the total diameter of the dryer

(
D t =D o +2 t i =1.32m+2 370.82 mm ×
1m
1000 mm )
D t =2.06 m

4.2.7 Calculation of the Live Load and Rotating Load

To calculate the volume of shell material:

π ( Do −D i ) L π ( 2.06 2−22 ) m2 ×6.8330 m

2 2

V SM = = =1.31 m3
4 4

To calculate the volume of insulating material:

π ( D o2−D i2 ) L π ( 2.06 2−1.322 ) m2 ×6.8330 m

V ℑ= = =13.37 m3
4 4

To calculate the weight of unloaded dryer using the density of mild steel 7850kg/m3

3 kg
W dryer =1.31 m ×7,850 =10,283.5 kg
m3

To calculate the weight of insulating material using the density of brick 2165kg/m3

3 kg
W insulation =13.37 m × 2,165 =28,946.05 kg
m3

To calculate the weight of the material in the dryer:

(
W material = 550.5535
kg
hr)×89.2775 min ×
1hr
60 min
=819.20 kg=1,806 Ibs

To calculate the total weight of the loaded dryer:

42
W total =10,283.5 kg+28,946.05 kg=39229.55 kg=86486.35 Ibs

4.2.8 Calculation of Blower Power, Motive Power and Power to Drive a Dryer

Using the equation in (van’t Land, 2012) for the calculation of motor power for rotation for

rotary dryers:

2
0.3 π Di L 0.3 π 2
P m= = × ( 2 ) × ( 6.8330 )
4 4

Pm=6.43 kW

To calculate the power requirement for blower:

( )( )( )
3
kg 1 kmol Pa. m
150 8,314 ( 372.77 K )
nRT hr 28.5740 kg kmol . K
Qinlet air = =
P 101,325 Pa

m3
Qinlet air =160.57
hr

Pb=2.72×10−5 Q inlet air p=2.72 ×10−5 ( 160.57 ) ( 20 )=0.0874 kW

Using the following equation proposed by CE Raymond Division, Combustion Engineering

Inc., to calculate the power to drive a dryer with flights (Mujumdar, 2014):

N ( 4.75 Di W material + 0.1925 D W total +0.33 W total )

P D=
100,000

Where N: expressed in rpm D: D+2

Wmaterial, Wtotal: expressed in Ibs, Diexpressed in feet

43
 4.75 ( ( 4.75× 1.32× 1,806 ) + ( 0.1925 ×2 ×86486.35 ) + ( 0.33 × 86486.35 ) )
P D=
100,000

0.75 kW
P D=45140.73 bhp× =33855.54
1bhp

P D=33,855 kW

tion. Oxford: Else

DESCRIPTION OF DRYER
CLASSIFICATION
CRITERIA
1.Form of Feed: Wet Filter
Cake
2.Mode of Operation:
Continuous operation
3.Heating System: Steam-
heated air
4.Gas Flow Pattern in Dryer:
Cocurrent gas flow

44
DESCRIPTION OF DRYER
CLASSIFICATION
CRITERIA
1.Form of Feed: Wet Filter
Cake
2.Mode of Operation:
Continuous operation
3.Heating System: Steam-
heated air
4.Gas Flow Pattern in Dryer:
Cocurrent gas flow
DESCRIPTION OF DRYER
CLASSIFICATION
CRITERIA
1.Form of Feed: Wet Filter
Cake
45
2.Mode of Operation:
Continuous operation
3.Heating System: Steam-
heated air
4.Gas Flow Pattern in Dryer:
Cocurrent gas flow
DESCRIPTION OF DRYER
CLASSIFICATION
CRITERIA
1.Form of Feed: Wet Filter
Cake
2.Mode of Operation:
Continuous operation
3.Heating System: Steam-
heated air

46
4.Gas Flow Pattern in
Dryer:Co
current gas flo

47
48
 CHAPTER 5

SIMULATION

5.1 Simulation Software: Aspen Plus was chosen for this design because it is better suitable

for chemical process design, whereas HYSYS is better suited for hydrocarbon process design

and can also handle very complex processes like the manufacturing of solid products such as

zeolite.

5.2. Selection of Fluid Package: Since Zeolites are aluminosilicate solids with a negatively

charged framework of micropores into which molecules can be adsorbed for environmental

purification and to catalyse chemical reactions, the property method adopted was method

filter: chemical and the base method was solid.

5.3. Process Conditions

Table 5.1: Process Condition of Mixer1

Name Unit H2O NaOH MIX2-FED

Stream Class MIXCIPSD MIXCIPSD MIXCIPSD

Temperature C 25 25 25.00000006

Pressure bar 1 1 1

Mass Vapor 0 0 0

Fraction

Mass Liquid 1 0 0.178000298

Fraction

Mass Solid 0 1 0.821999702

Fraction

49
Mass Enthalpy kJ/kg -2454.802991 -10645.76916 -9187.774739

Mass Entropy kJ/kg-K -6.46697488 -3.869892211 -4.332173699

Mass Density kg/cum 994.6944877 2101.610948 1754.145598

Enthalpy Flow kJ/hr -2211198.162 -44283200 -46494398.16

Average MW 18.01528 39.99711 32.86015221

Mass Flows kg/hr 900.764 4159.69944 5060.46344

Volume Flow l/min 15.09280841 32.98818179 48.08099021

Table 5.2: Process Condition of Mixer2

Name Unit 1H2O MIX2-FED PELLETS RFEED

Stream Class MIXCIPSD MIXCIPSD MIXCIPSD MIXCIPSD

Temperature C 25 25.00000006 1000 86.16981423

Pressure bar 1 1 1 1

Mass Vapor 0 0 0 0

Fraction

Mass Liquid 1 0.178000298 0 0.703518893

Fraction

Mass Solid 0 0.821999702 1 0.296481107

Fraction

Mass kJ/kg -2454.802991 - -14530.89949 -

Enthalpy 9187.774739 5675.236364

Mass kJ/kg-K -6.46697488 - -1.652227479 -

Entropy 4.332173699 4.870578173

Mass Density kg/cum 994.6944877 1754.145598 3051.15594 1190.823646

Enthalpy kJ/hr -75337903.8 - -133008120.9 -

50
Flow 46494398.16 254840423.6

Average MW 18.01528 32.86015221 91.5346782 22.93879719

Mass Flows kg/hr 30690 5060.46344 9153.46782 44903.93126

Volume l/min 514.2282443 48.08099021 50 628.4716103

Flow

Table 5.3: Process Conditions for Zeolite 4A Formation Reactor

Name RFEED ZEO-4A

Stream Class MIXCIPSD MIXCIPSD

Temperature C 86.16981423 90

Pressure Bar 1 1

Mass Vapor Fraction 0 0.922909153

Mass Liquid Fraction 0.703518893 0

Mass Solid Fraction 0.296481107 0.077090847

Mass Enthalpy kJ/kg -5675.236364 -1171.403565

Mass Entropy kJ/kg-K -4.870578173 -0.181995778

Mass Density kg/cum 1190.823646 56.61700957

Enthalpy Flow kJ/hr -254840423.6 -52600625.16

Average MW 22.93879719 533.8277114

Mass Flows kg/hr 44903.93126 44903.93126

Volume Flow l/min 628.4716103 13218.62211

Table 5.4: Process Conditions for Mixer3

Name CaCl2-H20 ZEO-4A MIX

Stream Class MIXCIPSD MIXCIPSD MIXCIPSD

51
Temperature C 50 90 54.7664809

Pressure bar 1 1 1

Mass Vapor 0 0.922909153 0.846010011

Fraction

Mass Liquid 0.5 0 0.042308127

Fraction

Mass Solid 0.5 0.077090847 0.111681862

Fraction

Mass Enthalpy kJ/kg -4752.141059 -1171.403565 -1464.282882

Mass Entropy kJ/kg-K -3.759743821 -0.181995778 -0.467703621

Mass Density kg/cum 1350.831152 56.61700957 58.59939274

Enthalpy Flow kJ/sec -5280.156732 -14611.28477 -19891.4415

Average MW 30.99872071 533.8277114 229.4295243

Mass Flows kg/hr 4000 44903.93126 48903.93126

Volume Flow l/min 49.35233139 13218.62211 13909.11207

Table 5.5: Process Conditions for Zeolite 5A Formation Reactor

Name MIXCIPSD ZEO-5A

Stream Class MIXCIPSD MIXCIPSD

Temperature C 54.7664809 50

Pressure Bar 1 1

Mass Vapor Fraction 0.846010011 0.814097016

Mass Liquid Fraction 0.042308127 0.042854348

Mass Solid Fraction 0.111681862 0.143048636

Mass Enthalpy kJ/kg -1464.282882 -1671.160118

52
Mass Entropy kJ/kg-K -0.467703621 -0.543028421

Mass Density kg/cum 58.59939274 61.69170874

Enthalpy Flow kJ/hr -71609189.4 -81726299.51

Average MW 229.4295243 193.602428

Mass Flows kg/hr 48903.93126 48903.93126

Volume Flow l/min 13909.11207 13211.91352

Table 5.6: Process Conditions for Zeolite 5A-Dry Formation Reactor

Name ZEO-5A ZEO5A-R1

Stream Class MIXCIPSD MIXCIPSD

Temperature C 50 50

Mass Vapor Fraction 0.814097016 0.252565257

Mass Liquid Fraction 0.042854348 0.604386107

Mass Solid Fraction 0.143048636 0.143048636

Mass Enthalpy kJ/kg -1671.160118 -2979.538918

Mass Entropy kJ/kg-K -0.543028421 -3.972992043

Mass Density kg/cum 61.69170874 59.72789518

Enthalpy Flow kJ/hr -81726299.51 -145711166.4

Average MW 193.602428 27.59186397

Mass Flows kg/hr 48903.93126 48903.93126

Volume Flow l/min 13211.91352 13646.31247

Table 5.7: Process Conditions for Dryer

Name AIR-IN ZEO5A-IN AIR-OUT ZEO5ADR

53
Stream Class MIXCIPSD MIXCIPSD MIXCIPSD MIXCIPSD

Temperature C 190 50 99.61507212 99.61508601

Pressure bar 1.702725729 1 1 1

Mass Vapor 1 0.252565257 1 0

Fraction

Mass Liquid 0 0.604386107 0 0.770971915

Fraction

Mass Solid 0 0.143048636 0 0.229028085

Fraction

Mass Enthalpy kJ/kg 166.286298 -2979.538918 45.90779571 -

4149.167934

Mass Entropy kJ/kg-K 0.294557941 -3.972992043 0.267376422 -

4.726308978

Mass Density kg/cum 1.280141486 59.72789518 1.681927944 1094.204128

Enthalpy Flow kJ/hr 24942.94469 -145711166.4 849708.6851 -

126735932.4

Average MW 28.95090871 27.59186397 52.12785523 21.47245851

Mass Flows kg/hr 150 48903.93126 18509.02819 30544.90307

Volume Flow l/min 1952.909133 13646.31247 183410.8317 465.2529676

5.4. Process Simulation: The process simulation of the production of zeolite from kaolin

clay is given below.

54
Figure 5.1 Screenshot of Mass/Heat transfer of dryer

Figure 5.2 Screenshot of Specification of dryer

55
Figure 5.3 Screenshot of the setting of mixer1

Figure 5.4 Screenshot of the setting of kiln

56
Figure 5.5 Screenshot of the setting of mixer 3

Figure 5.6 Screenshot of the setting of Mixer 2

57
Figure 5.7 Screenshot of the specification of screen1

Figure 5.8 Screenshot of the specification of screen2

58
Figure 5.9 Screenshot of PSD of zeolite 4A formation reactor

Figure 5.10 Screenshot of Heat of Reaction of Zeolite 4A formation reactor

59
Figure 5.11 Screenshot of reaction tab of zeolite4A formation reactor

Figure 5.12 Screenshot of specification of zeolite4A formation reactor

60
Figure 5.13 Screenshot of PSD of zeolite 5A formation reactor

Figure 5.14 Screenshot of reaction tab of zeolite 5A formation reactor

61
Figure 5.15 Screenshot of the specification of zeolite 5A dry formation reactor

Figure 5.16 Screenshot of the PSD of zeolite 5A dry formation reactor

62
Figure 5.17 Screenshot of the specification of zeolite 5A dry formation reactor

Figure 5.18 PFD of actual zeolite 5A production.

63
 CHAPTER 6

PROCESS CONTROL AND INSTRUMENTATION

Instruments are provided to monitor the key process variables during plant operation. They

may be incorporated in automatic control loops, or used for the manual monitoring of the

process operation. They may also be part of an automatic computer data logging system.

Instruments monitoring critical process variables will be fitted with automatic alarms to alert

the operators to critical and hazardous situations.

It is desirable that the process variable to be monitored be measured directly; often, however,

this is impractical and some dependent variable, that is easier to measure, is monitored in its

place.

6.1 OBJECTIVES

The primary objectives of the designer when specifying instrumentation and control schemes

are:

1. Safe plant operation:

(a) To keep the process variables within known safe operating limits.

(b) To detect dangerous situations as they develop and to provide alarms and automatic shut-

down systems.

(c) To provide interlocks and alarms to prevent dangerous operating procedures.

2. Production rate: To achieve the design product output.

3. Product quality: To maintain the product composition within the specified quality

standards.

4. Cost: To operate at the lowest production cost, commensurate with the other objectives.

6.2 Selection of Controllers: At the heart of the entire process of achieving operational

excellence is selection of the right automation technologies that will ensure industrial

64
processes run smoothly at the desired level of performance. The cost of investment in

automation simply pales in front of selection of technology because the right technology will

respond quickly to the changing market dynamics and, consequently, ensure a sustainable

competitive advantage. The right technology selection will help minimize the total cost of

ownership over the life of your industrial facility as well as help to create a system, which has

the flexibility and capability to embrace the advancements of the future.

Thanks in large part to rapid advancements in controller technology, the functionalities are

merged, and the lines between various technologies are blurred. Over the last few years,

integrated safety has become a key differentiator and is among the most important selection

criteria for programmable logic controllers (PLCs). In the future, we will see even more

functions being integrated into PLC platforms like cyber security, which is currently

considered as a separate entity. 

Hence, selection of the best technology is not as easy as it once was, whether it is for some

Greenfield job or Brownfield job requiring an upgrade or a migration strategy for an entire

plant. In the past, the strengths and weaknesses of various systems were well known and

understood thus making the selection fairly easy. Not anymore.

We understand the challenge companies have in selecting and implementing a solution that

will best meet their plant-wide requirements. The criteria listed below will allow those

involved in the selection of the control system to make quick and improved decisions to meet

the exact control and business requirements.

The criteria

1. Integration with current installed base

The existing installed base is one of the prime considerations when selecting a control

system. Certain controller products may not be compatible with others. Making sure existing

products are compatible with any new products will save time and money.

65
2. Integration with business systems’ capabilities and limitations

Business systems are part of management reporting tools, and most companies use these.

Control systems should have capabilities to work with various business system applications

currently available in market. Most of such applications now work on open protocols like

open connectivity (OPC). So control systems have to be at least OPC-compliant.

3. Availability of support, training, and spares

Companies face a lot of issues if they decide to use a control system that is a low-cost but

unreliable brand. Brand reliability is very important, and existing customer profiles of

potential brands should be available while doing the decision making part. Customer

feedback and support mechanism details should be clearly checked. In addition to this, the

training options and future spare parts’ lifecycles should also be known.

4. Product lifecycle and obsolescence

Product lifecycle details should be available during the decision-making process.

Additionally, the obsolescence of product is a major aspect to be covered while selecting a

control system as this can have a financial impact if an upgrade or migration to a newer

product is required. 

5. Standards compliance

We have too many standards available in the market, and manufacturers are rapidly certifying

themselves on these standards to promote their product features. Compliance requirement

should be clear so as to look for the product having that specific compliance; e.g., if the

requirement is to have a SIL3-certified system then you should only be looking for SIL3

systems rather than a general purpose PLC.

6. Environmental considerations

Certain environments may affect the operation of a controller. For example, typical

controllers have an operating temperature of 32 to 130 F. If your application will include any

66
extreme environmental conditions, or you have specific codes at your facility that must be

met, you will need to either research products that meet those specifications or design the

installation to meet requirements. 

7. Robust design and architecture

The selected vendor should have a robust architecture of his product line. This is very useful

when expanding the system and its features in the future. This helps to select the required

feature or product category from the same vendor having ease of integration rather than

selecting a new manufacturer and putting yourself in a difficult situation. 

8. Reliability and scalability

The control system should be reliable; this can be checked from its current users. It has to

have a prominent user base. Moreover, it should have scalability in terms of expansion; i.e., it

should have sufficient expandability limitations to cater your future needs. 

9. Ease of deployment and maintenance

Deployment should be easy, having user-friendly interface supported by decent operating

manuals and documentation. This helps people work and maintain the system in a better

way. 

10. Overall cost of ownership and viability in the long run or return on investment

(ROI)

This is one the most important points and is fully linked with financial numbers. The budget

to be consumed or allocated for meeting the requirements through a control system should

have a well-defined and documented ROI otherwise you might have to revisit the

requirements to make the ROI heavy enough to defend the budgets.

67
6.3 Core Technical Aspects to be Determined Before Selecting a Control System

Sizing a PLC is critical to the success of your project. Too small and you may max out your

I/O on changes and additions. Too large and you may blow your budget. Make sure you leave

room for expansion but don’t break the bank. 

Control system features to be considered include:

 Program memory requirement (estimated memory required for program)

 Scan time requirement (e.g., for safety applications, faster scan times are

required)

 Memory backup requirement (memory backup through battery for a period of

time in case of power outage to control system)

 Simplex or redundant controllers

 Simplex or redundant I/O modules

 Simplex or redundant communication network

 Programming functions that are required (proportional-integral-derivative

(PID), calculations, etc.)

 Local or remote I/O module capability (whether I/O modules will be local

with PLC controller or remotely installed in field)

 User’s communication requirements (number/purpose/limitations of

communication ports available on PLC, protocols supported like Ethernet, Modbus,

and RS232, etc.)

 User’s programming language requirements (Ladder Logic, SFC, ST, FBD, C

Language, etc.).

68
6.3.1 Temperature Indicating Controller

Introduction

Temperature, pressure, flow, and level are the four most common process variables.

Temperature is important because it provides a critical condition for processes such as

combustion, chemical reactions, fermentation, drying, distillation, concentration, extrusion,

crystallization, and air conditioning. Poor temperature control can cause major safety, quality,

and productivity problems. Although highly desirable, it is often difficult to control the

temperature because its measurement must be within a specified range of accuracy and have a

specified degree of speed of response, sensitivity, and dependability. Additionally,

temperature measurements must also be representative of true operating conditions in order to

achieve successful automated control. The instrument selected, installation design, and

location of the measuring points determine these specifications.

Pressure indicator and controller will be installed to maintain the pressure drop across the

process.

69
 CHAPTER 7

EQUIPMENT COST AND ECONOMIC EVALUATION

7.1 Equipment Cost

Name Equipment Cost [USD]

ZEO4A-F 107400

SCREEN1 18300

MIXER1 0

DRYER 14200

ZEO5A-F 49100

SCREEN2 18300

ZEO5A-R1 103800

MIXER3 0

MIXER2 0

KILN 0

BAR SCREEN 0

TOTAL 311100

70
7.1.1 Cost of Reactor

Figure 7.1 Based on purchase cost of miscellaneous equipment, cost factors for use. Cost

basis mid 2004

Reactor: Jacketed

Unit: Capacity, m3

Size range = 3-30, we choose 20

71
Cost constant C = $15000

Index (n) = 0.40

Material of construction: Carbon Steel

Ce=CSn

0.40
Ce=15000× 20 =$ 49716.81

7.1.2 Cost of Dryer

Using

Purchase Cost

n
Ce=CS

Where;

Ce – purchase equipment cost

S – Characteristic size parameter

C – Cost constant

n – Index for that type of equipment

72
 Figure 7.2 Dryer cost estimates

Dryer: Rotary

Unit: Area, m2

Size range = 5-30, but we choose 25

Cost constant = $35,000

Index (n) = 0.45

Material of construction: Direct Gas Fired

Purchase cost,
n
Ce=CS

0.45
Ce=35000× 25 =$ 148,984.5

73
7.1.3 Cost of Screen

Figure 7.3 Cost estimates for screen

Area = 60ft2 = 5.57m2

Cost constant = $60,000

Size exponent = 0.75

Module factor = 2.8

Factor: Double check = 1.6

Stainless steel = 1.25

Nickel alloy = 1.8

n
Ce=CS

Ce=60000× 5.570.75=$ 217,541.80

74
7.1.4 Summary of Costing for the Plant

Summary

Total Capital Cost [USD] 2993180

Total Operating Cost [USD/Year] 1694880

Total Raw Materials Cost [USD/Year] 0

Total Product Sales [USD/Year] 0

Total Utilities Cost [USD/Year] 66459.6

Desired Rate of Return [Percent/'Year] 20

P.O. Period [Year] 0

Equipment Cost [USD] 311100

Total Installed Cost [USD] 792800

7.1.4 Utility Cost

Utilities

Name Fluid Rate Rate Units Cost per Hour Cost Units

Electricity   97.826 KW 7.581515 USD/H

75
7.1.5 Installation Cost

InstallationCost =Purchase Price × Installation Factor

1. Installation factor of dryer ¿ 1.25−96 ; avg ; 1.64

InstallationCost =$ 148,984.5× 1.30=$ 193679.85

2. Installation factor of reactors ¿ 1.40−2.10; avg :1.70

Material factors:

316 stainless steel ¿ 1.2

Glass lined ¿ 0.8

Lead lined ¿ 0.7

Mild steel ¿ 0.6

Considering installation factor of 1.40

Installationcost =$ 49,716.81× 2.00=$ 99433.62

3. Installation factor of screen ¿ 1.45−2.27 ; avg : 1.85

Factor: Double check ¿ 1.6

Stainless steel¿ 1.25

Nickel alloy ¿ 1.8

Installationcost =$ 217,541.80× 1.50=$ 326,312.7

Total installation cost=$ ( 193679.85+99433.62+326,312.7 ) =$ 619,426.17

While the computer simulation costing is;

Name Installed Cost [USD]

76
ZEO4A-F 262600

SCREEN1 25500

MIXER1 0

DRYER 24200

ZEO5A-F 196200

SCREEN2 25500

ZEO5A-R1 258800

MIXER3 0

MIXER2 0

KILN 0

TOTAL 792800

7.2. Economic Evaluation: Economic evaluation is simply the process of measuring the cost

effectiveness. It is used to measure two parameters – cost and outcome (effect) for the purpose of

identifying the best course of action based on the evidence available.

7.2.1 Production Cost

Total Purchase Cost of major equipment items (PCE): This is obtained by adding the

purchase cost of all equipment in the plant.

PCE=3 Reactor+2 Dryer+ 2 Screen

PCE=3 × 49716.81+2 ×148984.50+2 ×217541.80=$ 882,203.03 ≈ $ 882,203

Total Physical Plant Cost (PPC)

PPC=PCE (1+ f 1+ … f 9 )

77
Using the data below for solid process type

f 1−equipmenterection=0.50

f 2−piping=0.20

f 3−instrumentation=0.10

f 4−electrical=0.10

f 5−building=0.05

f 6−utilities=0.25

f 7−storage=0.25

f 8−sitedevelopment=0.05

f 9−ancillarybuilding=0.30

Total=2.80

PPC=882,203 ( 1+2.80 ) =$ 3,352,371.4

Other functions will be included as;

f 10−DesignandEngineeering=0.20

'
f 11−Contractor sfee=0.05

f 12−Contigencies=0.10

7.2.2 Estimation of Fixed Capital Cost

FixedCapitalCost =PPC ( 1+ f 10+f 11+ f 12 )

¿ 3,352,371.4 ( 1+0.20+0.05+ 0.10 )=$ 4,525,701.39

78
7.2.3 Estimation OF Working Capital

Working Capital, allow 5% of fixed capital to cover the cost of the initial solvent charge will

be;

WorkingCapital=4,525,701.39× 0.05=$ 226,285.07

7.2.4 Total Investment and Return in Investment

The Total investment and return in investment required = FC + WC

That is;

FC – Fixed Capital

WC – Working Capital

Totalinvestmentandreturnininvestment =4525701.39+226285.07=$ 4,751,986.46

Or

From Summary of costing table using simulator values.

Using the format below to calculate the production cost of zeolite 5A plant, we have;

Figure 7.4 Summary of production cost

79
 Summary of Production Cost
Variable Costs
1. Utilities [USD/Year} 66459.6
2. Raw Materials [USD/Year] 250,000
3. Miscellaneous Materials 14965.9

Sub Total A 331,426

Fixed Cost
4. Fixed capital 2993180
5. Maintenance 149659
6. Capital Charge 299318
7. Insurance 29931.8
8. Local Taxes 59863.6
9. Royalties 29931.8

Sub Total B 568704.2

Direct Production Cost A+B 900,130
10 Sales expenses 225032.425
11. General overhead

Sub Total C 225032.425

Annual Production Cost = A+B+C 1,125,162

Production rate [kg/hr] 3.4267

Production Cost [USD/kg-hr] 328351.5117

80
 CHAPTER EIGHT

SAFETY, ENVIRONMENT AND HAZOP

8.1 Safety

Safety is the condition of being protected against any danger. Every organization has a legal

and moral obligation to safeguard the health and welfare of its employees and the general

public. The good management practices needed to ensure safe operation will also ensure

efficient operation. In a chemical processing industry, the chemicals used or produced can be

hazardous to humans or the environment if not properly handled and this could equally lead

to a lot of damage structurally and financially.

The best organizations are those that have come to the realization that provision of safety is

not only the right thing to do for their employees, it is also profitable.

Advantages of a safe working environment

i. Ultimately, safety leads to more profit as less money is spent taking care of legal bills,

hospital bills, and repair of equipment.

ii. It gives the company a good name.

iii. Happy employees which increases their job performance.

Safety is usually considered in three classes:

i. Environment safety

ii. Personnel safety

iii. Plant and equipment safety.

A. Environment Safety

81
There are several hazards associated with industrial process. These hazards need to be

prevented and kept in check in order to protect the environment. Environment in this context

refers to the immediate surroundings around the plant. For the safety of the environment to be

ensured, the following points should be noted and applied;

i. Flaring of gases should be done minimally.

ii. The level of toxicity of effluent should be monitored regularly and kept in check.

iii. Storage tanks should be situated in areas away from vehicle traffic.

iv. The control room should be attended to at all times to ensure that there is an

immediate response if an alarm is triggered.

v. There should be a way of informing the community around the facility if there is

danger that might affect them e.g Fire. An alarm is suggested, and this should be

tested regularly.

vi. Protect pipe racks and cable trays from fire.

vii. Fire-fighting system must be provided within the complex. This consist:

a. Fire water pipe network throughout the facility supported by necessary hydrants.

Hoses should be permanently placed near these hydrants.

b. The system should have a suitable water pump. It is advised that there be at least 2

pumps. One big one to fill the lines or pump large volume of water into it (when the

water is being depleted very fast like in a case of fire) and a smaller jockey pump to

maintain the pressure in the line. It would start more frequently than the big pump.

c. It is suggested that the system should have its own separate standby generator.

d. Fire entry suits and other protective clothing, compressed air breathing apparatus and

fire blankets should be made available in every building.

B. Personnel Safety

82
 The personnel of a company refers to the operators and staff of that company who ensure that

the production process move on smoothly. Their safety can be ensured in the following was.

i. Provision of personal protective equipment (PPE) and ensuring that they are properly

used.

ii. Pipes and equipment that contain very hot liquids for example the heater must be

lagged to make sure it does not cause injury to personnel.

iii. All chemicals in the plant must be properly label with its chemical hazard

identification chart and their Material Safety Data Sheet (MSDS) must be available

and updated regularly also.

iv. First aid kits must be provided in all buildings.

v. Emergency means of transportation must be provided in case of any accident.

vi. Emergency exit doors must be provided and these exits clearly marked for all to see.

vii. Cleanliness of the facility must be ensured at all times to avoid unnecessary risk or

accident.

viii. Smoking should be avoided in process area.

ix. Fire extinguishers must be made available at strategic points within the facility.

x. All ladders must have hand rails and personnel encouraged to use them whenever

climbing.

xi. Safety signs and symbols should be placed at hazardous area

83
8.2 HAZOP

Vessel: Mixer 1
Line: Stream H2O
Intention: To transfer a mixture of NaOH and steam to Mixer 2

Guide word Deviation Causes Consequences Action

No Flow Blocked Valve High Conc. Of Valve Maintenance

pellet

More Flow Faulty Valve Less Conc. Of Valve Maintenance

Pellet

Less Flow Partially blocked More Pellet Valve Maintenance

valve

Vessel: Mixer 2
Line: Stream Pellet
Intention: To transfer Kaolin Pellets to Calcinator
Guide word Deviation Causes Consequences Action

No Flow Blocked Valve High Conc. Of Valve Maintenance

NaOH and steam

More Flow Faulty Valve Less Conc. Of Valve Maintenance

NaOH and steam

Less Flow Partially blocked More NaOH and Valve Maintenance

valve Steam

Vessel: Reactor

Intention: To Calcine a mixture of Kaolin Pellets, steam and NaOH to Metakaolin

84
Line: Stream ZEO-4A
Intention: To transfer Calcinator effluent to Mixer 3
Guide word Deviation Causes Consequences Action

No Flow Blocked Valve More CaCL-H20 Valve maintenance

More Flow Faulty Valve Less CaCL-H20 Valve maintenance

Less Flow Partially blocked More CaCL-H20 Valve maintenance

valve

As well as Composition Refractory particle Poisoning of Coat reactor

from reactor Mixture properly

Vessel: Mixer 3

Line: Stream 11

Intention: To transfer mixture of Zeolite 4A and CaCL-H2O to Reator

Guide word Deviation Causes Consequences Action

No Flow Blocked Valve No reation Valve

maintenance/Fix

Temperature alarm

Vessel: Reactor
Line: Stream Zeolite-5A
Intention: to transfer reactor effluent product to dryer
Guide word Deviation Causes Consequences Action

As well as Composition Refractory particle Poisoning of Coat reactor

from reactor Mixture properly

Vessel: Dryer

85
Line: Stream Air-in
Intention: To transfer air to dryer
Guide word Deviation Causes Consequences Action

No Flow Blocked Valve Wet reactor effluent Valve

product in the dryer maintenance/Fix

outlet Temperature/pressure

alarm

More Flow Faulty Valve Valve maintenance

Fix

Temperature/pressure

alarm

Less Flow Partially blocked Partially Wet Valve maintenance

valve reactor effluent Fix

product in the dryer Temperature/pressure

outlet alarm

Vessel: Dryer
Line: Stream ZEO5ADRY
Intention: To transfer Dry Zeolite 5A to Screener
Guide word Deviation Causes Consequences Action

No Flow Blocked Valve No Screening Valve

maintenance/Fix

Temperature/pressure

alarm

Vessel: Screen
Intention: To screen
Line: 5A- PSS

86
Intention: to transfer screened product to Kiln
Guide word Deviation Causes Consequences Action

No Flow Blocked valve No kilning Valve Maintenance

As well as Composition Improper Screening Tube plugging Maintenance/

Vessel: Kiln
Intention: to vent off H2O
Line: Stream SCREENIN
Intention: To transfer kilning effluent to Screener
Guide word Deviation Causes Consequences Action

No Flow Blocked valve No screening Valve Maintenance

As well as Composition Improper Kilning Maintenance/

8.3 Environmental Impact Assessment (EIA)

A. Hazard/Toxicological information

LD50: It was not possible to establish the value of acute oral LD 50. No animal died after a dose

of 20000 mg/kg. Higher doses may not be applied. It was not possible to establish the value

of acute dermal LD50. After the application of a dose of 5000 mg/kg onto the bare skin on the

back of experimental animals, no animal dies. Higher doses may not be applied.

Eye irritation: A very mild and short irritation of conjunctival membrane. (Besides a mild

repletion after 2 hours after the preparation application disappearing after 24 hours, no

inflammatory changes of conjunctival membrane were observed).

Skin irritation: Zeolite does cause any inflammatory changes on the intact or disturbed, no

other symptoms of toxicity even after a multiple application.

87
Affecting live organisms: Zeolite may be classified as a little toxic, even harmless substance.

It does not present any risk after repeated skin applications and is not absorbed by skin in

hazardous quantities. Irritation of conjunctival membrane is very mild and short lasting.

Waste Disposal:Mechanically, may be combined with soil as zeolite is a certified soil

excipient. Zeolite does not contaminate water – it may be drained into the sewage. Zeolite is

not a dangerous waste. Used packs of zeolite are to be salvaged or burnt in an approved

incinerator after being thoroughly emptied.

88
 CHAPTER 9

CONCLUSION AND RECOMMENDATION

9.1 Conclusion

The zeolite is a promising concept that ensures the long term stability of global energy

supply. The main challenge is to figure out a cost-effective solution in producing catalyst for

production of detergent and other petrochemicals in large quantities to meet consumers’

demands.

The aim of this work was to design a plant for the production of 30,000 kg/annum of zeolite

from kaolin clay. A comprehensive literature review was carried out to determine the

realization of the functions of the sub processes in the basis of design. The identified

processes were simulated using Aspen Plus software. The results of this simulation are

interpreted to answer the main posed at the beginning although the results were available with

warnings.

However, the aim of this work was achieved with few warnings. Aspen PLUS was used to

simulate the plant capable of producing 30,000 kg/annum of zeolites from kaolin clay. The

major steps took in process design consisted of technology selections and flow-sheet. The

heat and material balance data obtained from simulation results were used to perform

equipment sizing, equipment cost/ physical plant cost developments and an economic

decision was drawn as to the total capital required and most importantly the rate of return.

9.2 Recommendation

For the continuation and further expansion of this conceptual design, the author would like to

make the following recommendations as future steps.

89
 i. In order for this process to gain further attractions within the petrochemical

industries, it is highly recommended to look for additional steps to reduce costs. The

main cost lies in getting high yield of zeolites with desired particle size distribution.

ii. To seek for better and easiest ways of achieving zeolites within a short period of

time.

90
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